CN107055610B - It is a kind of to prepare even microballoon Na0.5Bi0.5TiO3The method of crystal - Google Patents
It is a kind of to prepare even microballoon Na0.5Bi0.5TiO3The method of crystal Download PDFInfo
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- CN107055610B CN107055610B CN201710397769.5A CN201710397769A CN107055610B CN 107055610 B CN107055610 B CN 107055610B CN 201710397769 A CN201710397769 A CN 201710397769A CN 107055610 B CN107055610 B CN 107055610B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
- C01G29/006—Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
Even microballoon Na is prepared the invention discloses a kind of0.5Bi0.5TiO3The method of crystal, the method of the invention is using metal salt as raw material, it adds in organic solvent and mixed solution is made, it adds alkaline aqueous solution and prepares the oxyhydroxide precipitation of titanium and bismuth as reactant, it adds in suitable sodium hydrate aqueous solution and slurries is made, Na sources are provided and promote crystallization, 23 25h are kept the temperature at 175 ~ 185 DEG C, hydro-thermal reaction obtains bismuth sodium titanate nanometer grade uniform microsphere, and characteristic feature scale sphere diameter is about 100 150nm.The present invention realizes the synthesis of bismuth sodium titanate nanometer microballoon, and microballoon is distributed in perfect spherical shape and uniformity coefficient is high, and radius of sphericity is easy to control, and technical process implementation is very convenient, of less demanding to experimental facilities, and at low cost, pollution is small, it is easy to accomplish large-scale production.The product can be used for preparing high performance piezoelectric ferroelectric ceramics, in fields Bright Prospects such as detector, energy converter, electro-optical device, photovoltaic device, mechanical-electric coupling devices.
Description
Technical field
The present invention relates to a kind of bismuth-sodium titanate Na with perovskite-like structure0.5Bi0.5TiO3（Abbreviation NBT）Ferroelectric nano
The preparation method of carrying material belongs to inorganic non-metallic material preparation, piezoelectric ceramic technology field.
Background technology
Bi1/2Na1/2TiO3Ferroelectric material has the performance of spontaneous polarization in certain temperature range, while has piezoelectricity again
Property, it is a kind of extremely important multifunctional material.Bismuth-sodium titanate base piezoelectric ceramic is since it is with ferroelectricity is strong, dielectric constant is small
（240~340）, acoustical behavior is good and remanent polarization is big（Pr=38µC/cm2）, and it is excellent with higher Curie temperature etc.
Point.For many years, it is always one of advanced function material and the hot spot of intellectual material research field.
Traditional ferroelectric piezoelectric functional material is mostly with leaded lead zirconate titanate（PZT）Based on based material, main component oxygen
It is to have toxicity and volatile substance to change zirconium, can bring harm to ecological environment and health.Its volatility can also make
Material nonstoichiometry is obtained, reduces material property.Bi1/2Na1/2TiO3As the green material of new development, further exploitation is high
The Bi of performance1/2Na1/2TiO3There is very important scientific meaning and urgent market to need for electronic material ceramics, film etc.
It asks.
Bi1/2Na1/2TiO3The shape of powder granule to the physical property of powder, chemical property, transport performance and craftsmanship
Can have a great impact.The dimensional effect of nanoparticle and apparent effect make the light for itself having not available for bulky grain material
Performance, generally existing " blue shift " phenomenon are learned, i.e. optical absorption band shifts to shortwave direction.Mobility, the fillibility of spherical nanoparticle
Good, powder forms ceramic material uniformity after combining is good.Uniform-spherical particle can also obtain low burning as ceramic material
Junction temperature, high consistency and consistent microstructure, narrow particle size distribution.Therefore, even grade is made
Spherical powder particle is the target that people pursue always.
Invention content
The purpose of the present invention is to provide a kind of uniform microsphere nanoscale sodium bismuth titanate crystal and a kind of simply and effectively systems
The method of standby spherical nanoscale sodium bismuth titanate crystal, with solve powder particle size existing for existing preparation method it is uneven,
The problem of pattern is poor.This method is easy to operate, simple for process, and cost is relatively low, passes through the selection and optimization to process conditions, gained
The nanometer degree of crystal, sphericity are greatly improved.
The present invention provides a kind of spherical nanoscale sodium bismuth titanate crystals, which is characterized in that affiliated crystal grain is uniform
Spherical, diameter are about 100-150 nm.
The present invention provides a kind of methods that ball shaped nano grade sodium bismuth titanate crystal particle is prepared by simple hydro-thermal method.It should
Method is with analytically pure Bi (NO3)3.5H2O be bismuth source, butyl titanate（Ti(OC4H9)4）For titanium source, while using NaOH as sodium
Source and mineralizer.First, by Bi (NO3)3.5H2After O is dissolved in a small amount of ethylene glycol monomethyl ether, addition solution of tetrabutyl titanate forms mixed
Solution is closed, certain time is stirred, is made into precursor solution, is put into 50ml and is lined in the hydrothermal reaction kettle of polyethylene liner, certain
Temperature and time under carry out hydro-thermal reaction.After reaction, product is washed repeatedly to neutrality with distilled water and alcohol
Afterwards, filtered, drying, grinding, finally obtain target powder.Above-mentioned preparation method includes the following steps：
（One）The preparation of presoma
（1）It is Bi in molar ratio:Ti =1.01~1.02:2 weigh Bi (NO3)3·5H2O, butyl titanate (Ti
(OC4H9)4), solvent is ethylene glycol monomethyl ether, prepares Na0.5Bi0.5TiO3A concentration of 0.2-1.5mol/L of Ti in precursor solution,
It is preferred that 0.5-1.5mol/L；
（2）Ammonium hydroxide is added dropwise while stirring, generates a large amount of precipitations, i.e. hydro-thermal presoma；
（3）Precipitation is filtered using Suction filtration device；A large amount of deionized waters, ethanol wash to acid-base value are in neutrality；
（4）The precipitation washed is placed in drying box at 80 DEG C after keeping the temperature 6 hours and taken out；It is heavy by dried white
Shallow lake need to be spare after grinding.
（Two）It is prepared by mineralising agent solution：The NaOH powder of corrresponding quality is weighed, prepares a concentration of 7.5-8.5 of NaOH solution
mol/L；The concentration of solution is preferably 8 mol/L.
（Three）Hydro-thermal reaction
（1）White precipitate after grinding is added in NaOH solution；
（2）It is placed on magnetic stirring apparatus and is vigorously stirred more than 12h, make solution to yellow slurry；
（3）Yellow slurry is poured into, 80% or so is filled into hydrothermal reaction kettle；
（4）Reaction kettle sealing is placed on 175-185 DEG C of heat preservation 23-25h in insulating box again；Preferred temperature is 180 DEG C,
Time is for 24 hours.
（Four）Post-processing
（1）Cooled to room temperature takes out hydrothermal reaction kettle after stopping heating；
（2）Flushing obtains the powdered precipitation of bottom after discarding the supernatant in reaction kettle；
（3）Precipitation deionized water and absolute ethyl alcohol are alternately washed, repeatedly；
（4）It is placed in drying box and processing is dried at 60-80 DEG C；
（5）Obtain the Na that powder is prepared0.5Bi0.5TiO3Ferroelectric nano powder.
In above-mentioned preparation method, the preparation method of precursor solution is：
（1）Ethylene glycol monomethyl ether is measured by precursor concentration demand, by Bi (NO3)3·5H2O solid materials are dissolved in the amount of weighing
In 1/3rd ethylene glycol monomethyl ether；It is 40-55 DEG C to keep temperature, magnetic agitation to Bi (NO3)3·5H2O is completely dissolved.Stirring
To solution in sticky clear solution, solution A is obtained；
（2）Ti (the OC that will be weighed again4H9)4/ 3rd ethylene glycol monomethyl ether is added in, stirs evenly, obtains solution B；
（3）Solution A is added in solution B, the ethylene glycol monomethyl ether for adding remaining 1/3rd rinses Ti (OC4H9)4
Corresponding solution A beakers, are conducted into B solution；Na after mixing0.5Bi0.5TiO3Ti's is a concentration of in precursor solution
Then solution is sufficiently stirred by 0.5mol/L ~ 1.5mol/L, precursor solution is filtered to obtain with ultrafiltration cup.
In the preparation process of above-mentioned precursor solution, by Bi (NO3)3∙5H2O is added in ethylene glycol monomethyl ether, stirring
30min-5h, until reaction is uniform.
In above-mentioned preparation method, Na0.5Bi0.5TiO3The concentration of Ti is preferably 1mol/L in precursor solution.
In above-mentioned preparation method, during using optimum condition, gained bismuth-sodium titanate powder granule sphericity highest, the most
Even, the ceramic material ferroelectric properties of preparation is best.
The present invention prepares that nanoscale is uniformly spherical, and diameter is about 100-150nm using hydro-thermal method.In the present invention
The condition of stringent control reaction, the deviation for having very little just can not prepare even-grained sphere.
The present invention uses solvent as ethylene glycol monomethyl ether in the preparation of presoma, different from Conventional solvents ethyl alcohol, while
A concentration of 7.5-8.5 mol/L, preferably 8 mol/L of sodium hydroxide are controlled, it is stringenter in the insulating process of hydro-thermal reaction
The temperature of control is 175-185 DEG C, the time is 23-25 hours, extends or the shortening reaction time will not all form uniform ball
Shape crystal.
Description of the drawings
Fig. 1 is the electron scanning image of gained bismuth-sodium titanate powder particle（SEM）.
Fig. 2 is the electron scanning image of gained bismuth-sodium titanate powder particle（SEM）.
Fig. 3 is the electron scanning image of bismuth-sodium titanate powder particle obtained by 220 DEG C of 24 h of heat preservation（SEM）.
Specific embodiment
With reference to specific embodiment, the present invention is described further, and the description below is only to play the role of explanation,
Limitation is not generated to the present invention.
Embodiment 1
（One）The preparation of precursor solution
（1）It is Bi in molar ratio:Ti =1.02:2 weigh Bi (NO3)3.5H2O, butyl titanate (Ti (OC4H9)4), according to
Ti weighs corresponding amount for 1 mol/L concentration；30ml ethylene glycol monomethyl ethers are measured again, by Bi (NO3)3·5H2O solids are placed in three points
One of ethylene glycol monomethyl ether（10ml）In；30 min are stirred on magnetic stirring apparatus, until Bi (NO3)3·5H2O is completely dissolved.It will claim again
Ti (the OC taken4H9)4/ 3rd ethylene glycol monomethyl ether is added in, pours into Bi (NO3)3·5H2In O solution, remaining second is added
Glycol methyl ether rinses Ti (OC4H9)4；Stirring makes stable yellow clear solution for a long time enough on magnetic stirring apparatus；
（2）Ammonium hydroxide is added dropwise while stirring（There to be a large amount of precipitation to generate）；Precipitation is utilized, funnel mistake is filtered by vacuum
Filter；It is washed to acid-base value and is in neutrality with a large amount of deionized waters；The precipitation washed is placed in drying box at 80 DEG C and keeps the temperature 6 hours
After take out；By dried white precipitate need to after grinding it is spare；
（Two）The preparation of mineralizer：Compound concentration is the NaOH solution 40ml of 8mol/L.
（Three）Hydro-thermal reaction
（1）White precipitate after grinding is added in NaOH solution；It is placed on magnetic stirring apparatus and is vigorously stirred more than 12h,
Solutions Solution is allowed to yellow slurry；
（2）Yellow slurry is poured into, 80% or so is filled into hydrothermal reaction kettle；Reaction kettle sealing is placed on drying box again
In 180 DEG C heat preservation for 24 hours.
（Four）Post-processing
Cooled to room temperature takes out hydrothermal reaction kettle after stopping reaction；It discards to rinse after the supernatant in reaction kettle and obtain
The powdered precipitation of bottom；Precipitation deionized water and absolute ethyl alcohol are alternately washed, repeatedly；80 DEG C are placed in drying box
Under processing is dried；Obtain the Na that powder is prepared0.5Bi0.5TiO3Ferroelectric nano powder.
Fig. 1 is the electron scanning image of 1 gained bismuth-sodium titanate powder particle of embodiment（SEM）, it is in figure it can be seen that uniform
Spheric granules.It can be seen that particle is evenly distributed and fine and close from the SEM figures of surface, granular size is basically identical.
Fig. 2 is the electron scanning image of gained bismuth-sodium titanate powder particle（SEM）, it can be seen that uniform spherical in figure
The scale of grain is in 100-150 nm or so.
Comparative example 1
Reaction kettle 175 DEG C of 24 h of heat preservation in insulating box, remaining condition is the same as embodiment 1.Obtained spherical bismuth-sodium titanate ratio
The diameter that embodiment 1 obtains is small.The reason is that reaction temperature reduces, the growth of crystal is affected.
Comparative example 2
Reaction kettle 180 DEG C of 22 h of heat preservation in insulating box, remaining condition is the same as embodiment 1.Obtained spherical bismuth-sodium titanate ratio
The diameter that embodiment 1 obtains is small.The reason is that the reaction time reduces, the growth of crystal is affected.
Comparative example 3
Reaction kettle 180 DEG C of 20 h of heat preservation in insulating box, remaining condition is the same as embodiment 1.Obtained spherical bismuth-sodium titanate ratio
The diameter that embodiment 1 obtains is small, and crystallinity also decreases.The reason is that the reaction time is short, the growth of crystal is affected, is grown
It is not enough.
Comparative example 4
When the concentration of mineralizer is changed to 6-7 mol/L, remaining condition is the same as embodiment 1.Obtained bismuth-sodium titanate particle does not have
Regular shape, particle is extremely uneven, and stick to each other is disperseed not open.
Comparative example 5
When the concentration of mineralizer is changed to 9 mol/L, remaining condition is the same as embodiment 1.Wadding is presented in obtained bismuth-sodium titanate particle
Shape mushroom cloud-like, particle is extremely uneven, and stick to each other is disperseed not open.
Comparative example 6
Reaction kettle 200 DEG C of 32 h of heat preservation in insulating box, remaining condition is the same as embodiment 1.Obtained spherical bismuth-sodium titanate
Grain is extremely uneven, and stick to each other is disperseed not open, and has larger single crystal growth under cotton-shaped wrappage, and octahedral shape is presented.
Comparative example 7
Reaction kettle 220 DEG C of 32 h of heat preservation in insulating box, remaining condition is the same as embodiment 1.Obtained spherical bismuth-sodium titanate
Grain is uneven, and stick to each other is disperseed not open, and spherical particle is encircled by larger monocrystal and formed.Fig. 3 is 220 DEG C of 24 h institutes of heat preservation
Obtain the electron scanning image of bismuth-sodium titanate powder particle（SEM）.
Comparative example 8
Solvent in forerunner's production procedure is changed to ethyl alcohol, other conditions are with embodiment 1, of obtained bismuth-sodium titanate
Grain is extremely non-uniform cube structure, granularity 15-55nm.
Claims (7)
1. a kind of prepare even microballoon Na0.5Bi0.5TiO3The method of crystal, it is characterized in that, include the following steps：
（One）The preparation of presoma
It is Bi in molar ratio:Ti =1.01~1.02:2 weigh Bi (NO3)3•5H2O, butyl titanate, solvent are ethylene glycol monomethyl ether,
Prepare Na0.5Bi0.5TiO3A concentration of 0.2mol/L ~ 1.5mol/L of Ti in precursor solution；Ammonium hydroxide is added dropwise while stirring, generates
A large amount of precipitations, i.e. hydro-thermal presoma；
（Two）It is prepared by mineralising agent solution：The NaOH powder of corrresponding quality is weighed, prepares a concentration of 7.5-8.5 of NaOH solution
mol/L；
（Three）Hydro-thermal reaction
Presoma after grinding is added in NaOH solution；It is placed on magnetic stirring apparatus and is vigorously stirred more than 12h, make solution to Huang
Mill base liquid；Yellow slurry is poured into, 80% is filled into hydrothermal reaction kettle；Reaction kettle sealing is placed in insulating box 180 DEG C again
23-25 h are kept the temperature, obtain a nanometer Na0.5Bi0.5TiO3Crystal.
2. according to the method described in claim 1, it is characterized in that, Na0.5Bi0.5TiO3Crystal is uniform-spherical, a diameter of 100-
150nm。
3. method according to claim 1 or 2, it is characterized in that：Prepare mineralising agent solution when, mineralising agent solution it is a concentration of
8 mol/L。
4. method according to claim 1 or 2, it is characterized in that：During hydro-thermal reaction, holding temperature is 180 DEG C, soaking time
For for 24 hours.
5. according to the method described in claim 1, it is characterized in that：The preparation method of precursor solution is：
（1）Ethylene glycol monomethyl ether is measured by precursor concentration demand, by Bi (NO3)3•5H2O solid materials are dissolved in the required of the amount of weighing
In the ethylene glycol monomethyl ether of total amount 1/3rd；It is 40-55 DEG C to keep temperature, magnetic agitation to Bi (NO3)3•5H2O is completely dissolved,
Stirring, in sticky clear solution, obtains solution A to solution；
（2）Ti (the OC that will be weighed again4H9)4/ 3rd ethylene glycol monomethyl ether is added in, stirs evenly, obtains solution B；
（3）Solution A is added in solution B, the ethylene glycol monomethyl ether for adding remaining 1/3rd rinses Ti (OC4H9)4It is corresponding
Solution A beaker, is conducted into B solution；Na after mixing0.5Bi0.5TiO3A concentration of 0.5mol/L of Ti in precursor solution ~
Then solution is sufficiently stirred by 1.5mol/L, precursor solution is filtered to obtain with ultrafiltration cup.
6. according to the method described in claim 5, it is characterized in that：A concentration of 1 mol/L of Ti in precursor solution.
7. according to the method described in claim 6, it is characterized in that：Step（1）In, Bi：The molar ratio of Ti is 1.02：2.
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| CN109160540A (en) * | 2018-08-14 | 2019-01-08 | 沈阳工业大学 | A kind of method that two one-step hydrothermals prepares bismuth-sodium titanate spherical powder |
| CN109225193B (en) * | 2018-09-21 | 2021-03-30 | 陕西师范大学 | Semiconductor photocatalytic material Na0.23TiO2Preparation method of (1) |
| CN109399708A (en) * | 2018-12-29 | 2019-03-01 | 陕西科技大学 | A kind of spherical bismuth-sodium titanate powder and preparation method thereof of hydro-thermal method preparation |
| CN111569934A (en) * | 2020-06-29 | 2020-08-25 | 济南大学 | Preparation method of bismuth iron niobate/graphite phase carbon nitride composite photocatalyst |
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| CN101525239A (en) * | 2009-04-22 | 2009-09-09 | 南京工业大学 | Method for synthesizing Bi0.5Na0.5TiO3 spheroidal particles by microwave hydrothermal method |
| CN101565203A (en) * | 2008-04-23 | 2009-10-28 | 中国科学院合肥物质科学研究院 | Bismuth sodium titanate nanometer flower and preparation method thereof |
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| JPH0699153B2 (en) * | 1985-11-28 | 1994-12-07 | ソニー株式会社 | Method for producing fine particles of sodium bismuth titanate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565203A (en) * | 2008-04-23 | 2009-10-28 | 中国科学院合肥物质科学研究院 | Bismuth sodium titanate nanometer flower and preparation method thereof |
| CN101525239A (en) * | 2009-04-22 | 2009-09-09 | 南京工业大学 | Method for synthesizing Bi0.5Na0.5TiO3 spheroidal particles by microwave hydrothermal method |
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| 水热法制备钛酸铋钠粉体及其生长机理研究;徐明珠等;《人工晶体学报》;20140131;第43卷(第1期);第68-73页 * |
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